Sodium Hydroxide → [4-(1-Methylpiperidin-4-ylidene)-4,10-dihydro-9-oxa-3-thiabenzo[f]azulen-6-ylsulfanyl]acetic acid

HRID 389033ノート

反応式

HRID 389033 の反応式
[OH-].[Na+].C[O:4][C:5](=[O:29])[CH2:6][S:7][C:8]1[CH:9]=[CH:10][C:11]2[O:20][CH2:19][C:18]3[CH:17]=[CH:16][S:15][C:14]=3[CH:13]([CH:21]3[CH2:26][CH2:25][N:24]([CH3:27])[CH2:23][CH2:22]3)[C:12]=2[CH:28]=1>C(O)C>[CH3:27][N:24]1[CH2:25][CH2:26][C:21](=[C:13]2[C:12]3[CH:28]=[C:8]([S:7][CH2:6][C:5]([OH:29])=[O:4])[CH:9]=[CH:10][C:11]=3[O:20][CH2:19][C:18]3[CH:17]=[CH:16][S:15][C:14]2=3)[CH2:22][CH2:23]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 86649444Methyl[4-(1-methylpiperidin-4-yl)-4,10-dihydro-9-oxa-3-thiabenzo[f]azulen-6-ylsulfanyl]acetate

生成物 1

HCID 68490446[4-(1-Methylpiperidin-4-ylidene)-4,10-dihydro-9-oxa-3-thiabenzo[f]azulen-6-ylsulfanyl]acetic acid収率 50.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

An aqueous sodium hydroxide (1.4 g, 680 mmol) solution was added to an ethanol (40 mL) solution of the compound obtained in Example 24 (2.9 g, 6.7 mmol), and the mixture was refluxed while heating for 2 hours. After allowing the mixture to cool in the air, the solvents were distilled off under a reduced pressure, water was added to the residue, and the mixture was neutralized with hydrochloric acid. The precipitated crystals were separated by filtration and dried, to give 1.3 g (50%) of the captioned compound.

後処理

  1. temperaturethe mixture was refluxed
  2. temperaturewhile heating for 2 hours
  3. temperatureto cool in the air
  4. distillationthe solvents were distilled off under a reduced pressure, water
  5. additionwas added to the residue
  6. customThe precipitated crystals were separated by filtration
  7. customdried

出典と根拠

ORDレコード
ord-db03ff07f27a4a339233a45dfa203a32
出典データセット
uspto-grants-2013_02
特許番号
US08377967B2

反応ノート

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